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The work presented in this thesis provides new and detailed insight into the mechanism and the kinetics of the adsorption and electrooxidation of fuel cell relevant small organic molecules, such as CO, formic acid, ethanol as well as ethylene glycol and its oxidative intermediates. The measurements were performed in a novel in situ ATR-FTIR spectroscopy flow cell set-up, which had been further extended within this PhD work, by coupling it with on-line differential mass spectrometry. These experimental techniques, i.e. in situ ATR-FTIRS and/or in situ ATR-FTIRS/DEMS opened the possibility to follow and even quantify single reaction pathways within complex reaction networks.